US4798629A - Spin-on glass for use in semiconductor processing - Google Patents

Spin-on glass for use in semiconductor processing Download PDF

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Publication number
US4798629A
US4798629A US07/111,316 US11131687A US4798629A US 4798629 A US4798629 A US 4798629A US 11131687 A US11131687 A US 11131687A US 4798629 A US4798629 A US 4798629A
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United States
Prior art keywords
glass
spin
parts
volume
methyltriethoxysilane
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Expired - Fee Related
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US07/111,316
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Thomas E. Wood
Henry G. Hughes
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Motorola Solutions Inc
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Motorola Inc
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Priority to US07/111,316 priority Critical patent/US4798629A/en
Assigned to MOTOROLA, INC., SCHAUMBURG, ILLINOIS, A CORP. OF reassignment MOTOROLA, INC., SCHAUMBURG, ILLINOIS, A CORP. OF ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: HUGHES, HENRY G., WOOD, THOMAS E.
Priority to MYPI88000840A priority patent/MY100529A/en
Priority to JP63255049A priority patent/JPH01130536A/en
Priority to KR1019880013737A priority patent/KR890007407A/en
Application granted granted Critical
Publication of US4798629A publication Critical patent/US4798629A/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • H10W99/00—
    • H10P14/6922—
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • H10P14/6686—
    • H10P14/6342—
    • H10P14/6682—

Definitions

  • This invention relates, in general, to spin-on glass (SOG) and, more particularly, to thick film spin-on glass used in semiconductor processing.
  • spin-on glass is well known in the art of semiconductor processing but is limited in usable thickness.
  • the maximum thickness utilized for spin-on glass is approximately 2000 Angstroms. Using films thicker than this cause the glass layer to become highly stressed which results in cracks developing during processing. If a thicker glass layer is desired, it would have to be put down in multiple layers separated by chemical vapor deposition (CVD) oxide. Even using multiple layers, it has been found that the maximum thickness is 4000 Angstroms, or two layers of 2000 Angstroms each separated by the CVD layer. The reason for this limitation is that the lower SOG layer cannot support more than one additional SOG layer during processing.
  • present experimental spin-on glasses have a shelf life of approximately one month. This makes it difficult to maintain stocks of large quantities and is greatly effected by shipping or processing delays.
  • a further object of the present invention is to provide a spin-on glass that can be utilized as a thick film in semiconductor processing.
  • Another object of the present invention is to provide a spin-on glass having an improved shelf life.
  • Still another object of the present invention is to provide a spin-on glass having improved adhesion and wetting characteristics.
  • Yet another object of the present invention is to provide a spin-on glass preferably having between 11.0 and 9.0 atomic weight percent carbon.
  • a particular embodiment of the present invention consists of a spin-on glass comprising, by volume: 1.0 parts tetraethoxysilane (also known as tetraethylorthosilicate, TEOS), methyltriethoxysilane, and dimethyldiethoxysilane in a mixture which provides between 11.0 and 9.0 atomic weight percent carbon based on the hydrolyzed organo silane; 1.1 parts ethanol (EtOH, also known as ethyl alcohol); 0.0002 parts hydrochloric acid (HCl); and 0.26 parts water (H 2 O).
  • tetraethoxysilane also known as tetraethylorthosilicate, TEOS
  • methyltriethoxysilane methyltriethoxysilane
  • dimethyldiethoxysilane in a mixture which provides between 11.0 and 9.0 atomic weight percent carbon based on the hydrolyzed organo silane
  • EtOH also known as ethyl alcohol
  • spin-on glass films have been used for various purposes in semiconductor devices: insulation between multilayer metallizations; contouring steps in oxides or metals for improved step coverage; preventatives for auto-doping; back-filling packages; diffusion masks; and planarizing.
  • the maximum thickness of the present glass is approximately 2000 Angstroms. This requires that more than one layer of glass be deposited; which, in turn, requires an intermediate layer, such as a chemical vapor deposited (CVD) oxide, be deposited.
  • CVD chemical vapor deposited
  • Some recent thick film spin-on glasses have been attempted resulting in very soft glass which is inoperable in a semiconductor processing environment. These glasses have been found to have wetting problems which result in voids being left between the glass and the substrate. A further problem is in the ability to provide adhesion to the substrate. Many of the glass layers have been found to detach from the substrate during or after completion of processing. An additional problem is that the glass is unable to maintain its composition during subsequent processing. The softness of the glass leaves it subject to mechanical damage (scratches) and prone to damage from subsequent process chemicals.
  • One preferred embodiment of the present invention is a glass composition, comprising as the main ingredients: tetraethoxysilane (also known as tetraethylorthosilicate, TEOS)/methyltriethoxysilane/ dimethyldiethoxysilane in a 2/1/1 relationship.
  • tetraethoxysilane also known as tetraethylorthosilicate, TEOS
  • TEOS tetraethylorthosilicate
  • the compositon is then mixed with ethanol, hydrochloric acid, and water in the following parts measured by volume.
  • This provides a spin-on glass that is approximately 9.5 atomic weight percent of carbon. It should be noted that the above is the preferable mixture and that mixtures within the following ranges are acceptable.
  • the preferred ratio of tetraethoxysilane, methyltriethoxysilane, and dimethyliethoxysilane is 2/1/1.
  • the main objective is to achieve an atomic weight percent of carbon in a hydrolyzed organo silane between 25.0 and 8.0 and preferably between 11.0 and 9.0 percent. This may also be achieved through ratios of 2/2/1 and 2/1/2 as well as others.
  • This provides a thick film spin-on glass which provides single layer thicknesses of 10,000 Angstroms or more.
  • the spin-on glass has been found to have a stable shelf life of more than three months. This is greatly improved over the inconsistent shelf lives of experimental thick film spin-on glasses.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Formation Of Insulating Films (AREA)
  • Silicon Polymers (AREA)
  • Glass Compositions (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)

Abstract

A spin-on glass consisting of, by volume: 1.0 parts tetraethoxysilane (TEOS, also known as tetraethylorthosilicate), methyltriethoxysilane, and dimethyldiethoxysilane in a 2/1/1 ratio; 1.1 parts ethanol (EtOH, also known as ethyl alcohol); 0.0002 parts hydrochloric acid (HCl); and 0.26 parts water (H2 O).

Description

BACKGROUND OF THE INVENTION
This invention relates, in general, to spin-on glass (SOG) and, more particularly, to thick film spin-on glass used in semiconductor processing.
The use of spin-on glass is well known in the art of semiconductor processing but is limited in usable thickness. Presently, the maximum thickness utilized for spin-on glass is approximately 2000 Angstroms. Using films thicker than this cause the glass layer to become highly stressed which results in cracks developing during processing. If a thicker glass layer is desired, it would have to be put down in multiple layers separated by chemical vapor deposition (CVD) oxide. Even using multiple layers, it has been found that the maximum thickness is 4000 Angstroms, or two layers of 2000 Angstroms each separated by the CVD layer. The reason for this limitation is that the lower SOG layer cannot support more than one additional SOG layer during processing.
In addition, present experimental spin-on glasses have a shelf life of approximately one month. This makes it difficult to maintain stocks of large quantities and is greatly effected by shipping or processing delays.
Further, present attempts to make thick film spin-on glass are subject to: being detached from the substrate during normal chemical processing; or, simply falling off the substrate. These relate to adhesion and wetting problems.
Therefore, it is an object of the present invention to provide a spin-on glass that overcomes the above deficiencies.
A further object of the present invention is to provide a spin-on glass that can be utilized as a thick film in semiconductor processing.
Another object of the present invention is to provide a spin-on glass having an improved shelf life.
Still another object of the present invention is to provide a spin-on glass having improved adhesion and wetting characteristics.
Yet another object of the present invention is to provide a spin-on glass preferably having between 11.0 and 9.0 atomic weight percent carbon.
The above and other objects and advantages of the present invention are provided by the spin-on glass described herein.
SUMMARY OF THE INVENTION
A particular embodiment of the present invention consists of a spin-on glass comprising, by volume: 1.0 parts tetraethoxysilane (also known as tetraethylorthosilicate, TEOS), methyltriethoxysilane, and dimethyldiethoxysilane in a mixture which provides between 11.0 and 9.0 atomic weight percent carbon based on the hydrolyzed organo silane; 1.1 parts ethanol (EtOH, also known as ethyl alcohol); 0.0002 parts hydrochloric acid (HCl); and 0.26 parts water (H2 O).
DESCRIPTION
Spin-on glass films have been used for various purposes in semiconductor devices: insulation between multilayer metallizations; contouring steps in oxides or metals for improved step coverage; preventatives for auto-doping; back-filling packages; diffusion masks; and planarizing. In these applications, it is desirable for the spin-on glass to be of a thickness greater than many of the present commercially available materials can provide. The maximum thickness of the present glass is approximately 2000 Angstroms. This requires that more than one layer of glass be deposited; which, in turn, requires an intermediate layer, such as a chemical vapor deposited (CVD) oxide, be deposited.
Some recent thick film spin-on glasses have been attempted resulting in very soft glass which is inoperable in a semiconductor processing environment. These glasses have been found to have wetting problems which result in voids being left between the glass and the substrate. A further problem is in the ability to provide adhesion to the substrate. Many of the glass layers have been found to detach from the substrate during or after completion of processing. An additional problem is that the glass is unable to maintain its composition during subsequent processing. The softness of the glass leaves it subject to mechanical damage (scratches) and prone to damage from subsequent process chemicals.
One preferred embodiment of the present invention is a glass composition, comprising as the main ingredients: tetraethoxysilane (also known as tetraethylorthosilicate, TEOS)/methyltriethoxysilane/ dimethyldiethoxysilane in a 2/1/1 relationship. The compositon is then mixed with ethanol, hydrochloric acid, and water in the following parts measured by volume.
______________________________________                                    
Element                 Parts                                             
______________________________________                                    
Tetraethoxysilane/Methyltriethoxysilane/                                  
                        1.0                                               
Dimethyldiethoxysilane 2/1/1                                              
Ethanol                 1.1                                               
HCl                     0.0002                                            
H.sub.2 O               0.26                                              
______________________________________
This provides a spin-on glass that is approximately 9.5 atomic weight percent of carbon. It should be noted that the above is the preferable mixture and that mixtures within the following ranges are acceptable.
______________________________________                                    
Element                 Parts                                             
______________________________________                                    
Tetraethoxysilane/Methyltriethoxysilane/                                  
                        1.0                                               
Dimethyldiethoxysilane                                                    
Ethanol                 0.7-2.7                                           
HCl                     0.0001-0.004                                      
H.sub.2 O               0.05-0.40                                         
______________________________________
As shown in the first embodiment above, the preferred ratio of tetraethoxysilane, methyltriethoxysilane, and dimethyliethoxysilane is 2/1/1. However, the main objective is to achieve an atomic weight percent of carbon in a hydrolyzed organo silane between 25.0 and 8.0 and preferably between 11.0 and 9.0 percent. This may also be achieved through ratios of 2/2/1 and 2/1/2 as well as others.
This provides a thick film spin-on glass which provides single layer thicknesses of 10,000 Angstroms or more. In addition, the spin-on glass has been found to have a stable shelf life of more than three months. This is greatly improved over the inconsistent shelf lives of experimental thick film spin-on glasses.
Thus, it will be apparent to one skilled in the art, following a review of the above specification, that there has been provided in accordance with the invention, a spin-on glass that fully satisfies the objects, aims, and advantages set forth above.
While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alterations, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alterations, modifications, and variations in the appended claims.

Claims (20)

I claim:
1. A spin-on glass for use in processing semiconductor devices, said spin-on glass comprising:
a first compound of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane combined in a 2/1/1 ratio;
ethanol;
hydrochloric acid; and
water.
2. The spin-on glass of claim 1 wherein said 2/1/1 compound is 1.0 parts by volume of said spin-on glass.
3. The spin-on glass of claim 1 wherein said ethanol is 1.1 parts by volume of said spin-on glass.
4. The spin-on glass of claim 1 wherein said hydrochloric acid is 0.0002 parts by volume of said spin-on glass.
5. The spin-on glass of claim 1 wherein said water is 0.26 parts by volume of said spin-on glass.
6. The spin-on glass of claim 1 wherein a mixture of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane between approximately 25.0 and 8.0 atomic weight percent carbon based on hydrolyzed organo silanes.
7. The spin-on glass of claim 1 wherein a mixture of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane having between approximately 11.0 and 9.0 atomic weight percent carbon based on hydrolyzed organo silanes.
8. The spin-on glass of claim 1 wherein a mixture of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane having approximately a 9.5 atomic weight percent carbon based on hydrolyzed organo silanes.
9. A spin-on glass for use in processing a semiconductor device, said spin-on glass comprising:
a first compound, being 1.0 parts by volume, of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane in a 2/1/1 composition;
ethanol being between 0.1 and 2.7 parts by volume;
hydrochloric acid being between 0.0001 and 0.004 parts by volume; and
water being between 0.05 and 0.40 parts by volume.
10. The spin-on glass of claim 9 wherein said ethanol is 1.1 parts of said spin-on glass.
11. The spin-on glass of claim 9 wherein said hydrochloric acid is 0.0002 parts of said spin-on glass.
12. The spin-on glass of claim 9 wherein said water is 0.26 parts of said spin-on glass.
13. The spin-on glass of claim 9 wherein a hydrolyzed solution of said first compound comprises between approximately 25.0 and 8.0 atomic weight percent of carbon.
14. The spin-on glass of claim 10 wherein a hydrolyzed solution of said first compound comprises between approximately 11.0 and 9.0 atomic weight percent of carbon.
15. The spin-on glass of claim 9 wherein a hydrolyzed solution of said first compound comprises approximately 9.5 atomic weight percent of carbon.
16. A spin-on glass for processing semiconductor devices, said spin-on glass comprising:
a first compound being 1.0 parts by volume of said spin-on glass, said first compound comprising tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane in a 2/1/1 ratio;
ethanol being 1.1 parts by volume of said spin-on glass;
hydrochloric acid being 0.0002 parts by volume of said spin-on glass; and
water being 0.26 parts by volume of said spin-on glass.
17. A spin-on glass of claim 16 wherein a hydrolyzed solution of said first compound comprises between approximately 11.0 and 9.0 atomic weight precent of carbon.
18. A spin-on glass of claim 16 wherein a hydrolyzed solution of said first compound comprises approximately 9.5 atomic weight percent of carbon.
19. A spin-on glass for use in processing semiconductor devices, said spin-on glass comprising:
a first compound of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane combined in a 2/2/1 ratio;
ethanol;
hydrochloric acid; and
water.
20. A spin-on glass for use in processing semiconductor devices, said spin-on glass comprising:
a first compound of tetraethoxysilane, methyltriethoxysilane, and dimethyldiethoxysilane combined in a 2/2/1 ratio;
ethanol;
hydrochloric acid; and
water.
US07/111,316 1987-10-22 1987-10-22 Spin-on glass for use in semiconductor processing Expired - Fee Related US4798629A (en)

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US07/111,316 US4798629A (en) 1987-10-22 1987-10-22 Spin-on glass for use in semiconductor processing
MYPI88000840A MY100529A (en) 1987-10-22 1988-07-27 Spin-on glass for use in semiconductor processing
JP63255049A JPH01130536A (en) 1987-10-22 1988-10-12 Spin-on glass for semiconductor processing
KR1019880013737A KR890007407A (en) 1987-10-22 1988-10-21 Spin-on Glass for Semiconductor Processing

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Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0424638A3 (en) * 1989-08-31 1991-07-31 Fujitsu Limited Fabrication of a semiconductor device including a step for prodiving a layer of insulating material formed from an organo-silica sol
EP0474383A1 (en) * 1990-08-16 1992-03-11 Motorola, Inc. Dielectric for use in manufacturing semiconductors
US5152834A (en) * 1990-09-14 1992-10-06 Ncr Corporation Spin-on glass composition
US5302198A (en) * 1990-09-14 1994-04-12 Ncr Corporation Coating solution for forming glassy layers
US5472488A (en) * 1990-09-14 1995-12-05 Hyundai Electronics America Coating solution for forming glassy layers
US5510147A (en) * 1995-03-03 1996-04-23 International Paper Company Sol gel barrier films
US5527872A (en) * 1990-09-14 1996-06-18 At&T Global Information Solutions Company Electronic device with a spin-on glass dielectric layer
US5817582A (en) * 1991-02-04 1998-10-06 Motorola, Inc. Process for making a semiconductor device having a TEOS based spin-on-glass
US5840821A (en) * 1994-03-11 1998-11-24 Kawasaki Steel Corporation Coating solution and method for preparing the coating solution, method for forming insulating films for semiconductor devices, and method for evaluating the coating solution
US6054379A (en) * 1998-02-11 2000-04-25 Applied Materials, Inc. Method of depositing a low k dielectric with organo silane
US6214104B1 (en) * 1995-08-07 2001-04-10 Tokyo Ohka Kogyo Co., Ltd. Coating solution for forming silica coating and method of forming silica coating
US6268089B1 (en) * 1998-02-23 2001-07-31 Agere Systems Guardian Corp. Photorecording medium and process for forming medium
US6287990B1 (en) 1998-02-11 2001-09-11 Applied Materials, Inc. CVD plasma assisted low dielectric constant films
US6303523B2 (en) 1998-02-11 2001-10-16 Applied Materials, Inc. Plasma processes for depositing low dielectric constant films
US6399489B1 (en) 1999-11-01 2002-06-04 Applied Materials, Inc. Barrier layer deposition using HDP-CVD
US6423770B1 (en) 1999-07-15 2002-07-23 Lucent Technologies Inc. Silicate material and process for fabricating silicate material
US20030049388A1 (en) * 2001-09-10 2003-03-13 Seon-Mee Cho Silicon carbide deposited by high density plasma chemical-vapor deposition with bias
US6593655B1 (en) 1998-05-29 2003-07-15 Dow Corning Corporation Method for producing hydrogenated silicon oxycarbide films having low dielectric constant
US6593247B1 (en) 1998-02-11 2003-07-15 Applied Materials, Inc. Method of depositing low k films using an oxidizing plasma
US6660656B2 (en) 1998-02-11 2003-12-09 Applied Materials Inc. Plasma processes for depositing low dielectric constant films
US6667553B2 (en) 1998-05-29 2003-12-23 Dow Corning Corporation H:SiOC coated substrates
US6709721B2 (en) 2001-03-28 2004-03-23 Applied Materials Inc. Purge heater design and process development for the improvement of low k film properties
US20040166665A1 (en) * 1998-02-11 2004-08-26 Applied Materials, Inc. Method of decreasing the K value in SIOC layer deposited by chemical vapor deposition
US20070173074A1 (en) * 2000-02-02 2007-07-26 Min-Jin Ko Semiconductor interlayer dielectric material and a semiconductor device using the same

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Cited By (49)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0424638A3 (en) * 1989-08-31 1991-07-31 Fujitsu Limited Fabrication of a semiconductor device including a step for prodiving a layer of insulating material formed from an organo-silica sol
EP0474383A1 (en) * 1990-08-16 1992-03-11 Motorola, Inc. Dielectric for use in manufacturing semiconductors
US6274515B1 (en) 1990-08-16 2001-08-14 Motorola, Inc. Spin-on dielectric formation process for use in manufacturing semiconductors
US5527872A (en) * 1990-09-14 1996-06-18 At&T Global Information Solutions Company Electronic device with a spin-on glass dielectric layer
US5472488A (en) * 1990-09-14 1995-12-05 Hyundai Electronics America Coating solution for forming glassy layers
US5665845A (en) * 1990-09-14 1997-09-09 At&T Global Information Solutions Company Electronic device with a spin-on glass dielectric layer
US5302198A (en) * 1990-09-14 1994-04-12 Ncr Corporation Coating solution for forming glassy layers
US5152834A (en) * 1990-09-14 1992-10-06 Ncr Corporation Spin-on glass composition
US5817582A (en) * 1991-02-04 1998-10-06 Motorola, Inc. Process for making a semiconductor device having a TEOS based spin-on-glass
US5840821A (en) * 1994-03-11 1998-11-24 Kawasaki Steel Corporation Coating solution and method for preparing the coating solution, method for forming insulating films for semiconductor devices, and method for evaluating the coating solution
US5998522A (en) * 1994-03-11 1999-12-07 Kawasaki Steel Corporation Coating solution and method for preparing the coating solution, method for forming insulating films for semiconductor devices, and method for evaluating the coating solution
US5510147A (en) * 1995-03-03 1996-04-23 International Paper Company Sol gel barrier films
US5618628A (en) * 1995-03-03 1997-04-08 International Paper Company Sol gel barrier films
US6214104B1 (en) * 1995-08-07 2001-04-10 Tokyo Ohka Kogyo Co., Ltd. Coating solution for forming silica coating and method of forming silica coating
US6537929B1 (en) 1998-02-11 2003-03-25 Applied Materials, Inc. CVD plasma assisted low dielectric constant films
US20050156317A1 (en) * 1998-02-11 2005-07-21 Applied Materials, Inc. Low dielectric constant film produced from silicon compounds comprising silicon-carbon bonds
US6072227A (en) * 1998-02-11 2000-06-06 Applied Materials, Inc. Low power method of depositing a low k dielectric with organo silane
US6287990B1 (en) 1998-02-11 2001-09-11 Applied Materials, Inc. CVD plasma assisted low dielectric constant films
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